Water → HCID 13393463, compound

Participants

Reaction Steps

Potassium carbonate (11.4 mmole) was added to a solution of the product of Example 4 (5.7 mmole) in 50 ml xylene, heated to reflux, and the water formed removed with a Dean-Stark trap. After 1 hour the Dean-Stark trap was drained. The solution was cooled to room temperature and methyl p-toluenesulfonate (17.1 mmole) added. The solution was heated to 70° C. for 20 hours, and refluxed for one hour to remove the water formed. After the white solid was filtered and discarded, the filtrate was concentrated under vacuum to a solid, which was was recrystallized from hot hexane, to give the title compound (1.6 g), m.p. ca. 73°-74° C.

Provenance & Evidence